This invention relates to the preparation of a subhydride of titanium. More particularly, this invention relates to the preparation of a titanium subhydride of a selected titanium-hydrogen composition, the subhydride being of substantially uniform titanium-hydrogen composition.
In the prior art, it is known to prepare titanium subhydride for the purpose of developing pressure/temperature/composition diagrams. In this work, stoichiometric titanium hydride is heated under equilibrium vacuum conditions to a certain temperature, hydrogen gas coming off the titanium material is captured and the volume of the gas is measured. Illustrative of this type of prior art is Gibb, Jr. et al, "The Titanium-Hydrogen System and Titanium Hydride. I. Low-Pressure Studies", Journal of the American Chemical Society, Vol. 72, pp. 5365-5369 (1950). In this particular prior art reference, stoichiometric titanium hydride is evacuated briefly at 200.degree.-300.degree. C., following which pure hydrogen is obtained as needed by heating to above 500.degree. C. Also in this reference, the dissociation pressure was measured for the Ti-H system over the range 500.degree.-800.degree. C. at 50-800 mm. Also, it is known in the prior art to prepare fine powder of metals such as titanium using stoichiometric titanium hydride starting material by heating the starting material at a temperature higher than 500.degree. C. in a vacuum of 5.times.10.sup.-5 mm. Hg. Prior art of this type is exemplified by U.S. Pat. No. 3,376,107 to Oka.
This prior art and the other prior art of which I am aware is deficient since it fails to provide a process for reproducibly preparing titanium subhydride of a selected titanium-hydrogen composition. Also, this prior art fails to provide a process for producing a titanium subhydride of substantially uniform titanium-hydrogen composition. Furthermore, this art does not provide a process for providing a subhydride of substantially uniform titanium-hydrogen composition that is in the form of free-flowing, dust-free spheres of friable powder. Moreover, this art does not provide a process of the type described in which there is a minimum of sintering of the titanium starting material and of the subhydride.